1、Designation:D215805 Designation: D2158 11Designation: 317/95Standard Test Method forResidues in Liquefied Petroleum (LP) Gases1This standard is issued under the fixed designation D2158; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisio
2、n, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of extraneous materials weathering above 38C that are presen
3、t in liquefiedpetroleum gases.The extraneous materials will generally be dissolved in the LPG, but may have phase-separated in some instances.1.2 Liquefied petroleum gases that contain certain anti-icing additives can give erroneous results by this test method.1.3 Although this test method has been
4、used to verify cleanliness and lack of heavy contaminants in propane for many years,it might not be sensitive enough to protect some equipment from operational problems or increased maintenance.Amore sensitivetest, able to detect lower levels of dissolved contaminants, could be required for some app
5、lications.1.41.4 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that can cause centralnervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercur
6、y containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into your state or country may be prohibited by law
7、.1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish
8、appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D96 Test Methods forMethod For Water and Sediment in Crude Oil by Centrifuge Method (Field Procedure)Field Procedure3D1796 Test Method for Water an
9、d Sediment in Fuel Oils by the Centrifuge Method (Laboratory Procedure)D1835 Specification for Liquefied Petroleum (LP) GasesE1 Specification for ASTM Liquid-in-Glass Thermometers2.2 Other Document: Energy Institute Document:IPAppendix AIP Test Methods - Appendix A. Specifications - IP standard ther
10、mometers43. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 oil stain observation, nthe volume of solvent-residue mixture required to yield an oil stain or ring that persists for 2minutes under specified conditions on absorbent paper.3.1.2 residue, nthe volume, measured to the ne
11、arest 0.05 mL, of the residual material boiling above 38C resulting from theevaporation of 100 mL of sample under the specified conditions of this test method.3.1.3 solvent-residue mixture, na mixture (solution) of 10 mL of solvent with any residue remaining in the centrifuge tube1This test method i
12、s under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.H0 onLiquefied Petroleum Gas.Current edition approved Nov.Jan. 1, 2005.2011. Published November 2005.February 2011. Originally approved in 1963. Last previous edit
13、ion approved in 20042005 asD215804.D215805. DOI: 10.1520/D2158-05.10.1520/D2158-11.2For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page
14、 on the ASTM website.3Withdrawn.3Withdrawn. The last approved version of this historical standard is referenced on www.astm.org.4Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K. www.energyinstpubs.org.uk1This document is not an ASTM standard and is intended only to provid
15、e the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the st
16、andard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.at the conclusion of the first step in this test m
17、ethod.4. Summary of Test Method4.1 A 100-mL sample of liquefied petroleum gas is weathered in a 100-mL centrifuge tube. The volume of residue remainingafter heating the tube to 38C is measured and recorded.4.2 To dissolve any residue, 10 mL of solvent is added to the centrifuge tube. Small, measured
18、 volumes of solvent-residuemixture are deposited on an absorbent paper in a specified manner. The appearance of the absorbent paper to which the residuesolution has been added in measured increments is observed and recorded.5. Significance and Use5.1 Control over the residue content (required by Spe
19、cification D1835) is of considerable importance in end-use applicationsof LPG. In liquid feed systems residues can lead to troublesome deposits and, in vapor withdrawal systems, residues that are carriedover can foul regulating equipment. Those that remain will accumulate, can be corrosive, and will
20、 contaminate following product.Water, particularly if alkaline, can cause failure of regulating equipment and corrosion of metals.6. Interferences6.1 Solid contaminants such as rust, scale or dirt can interfere with this test method, which is not intended for representativemeasurement of solid, undi
21、ssolved contaminants.7. Apparatus7.1 Centrifuge Tube, 100-mL graduated, conforming to dimensions given in Fig. 1. The first 0.5 mL shall be graduated in0.05-mL increments. The shape of the lower tip of the tube is especially important. The taper shall be uniform and the bottom shallbe rounded as sho
22、wn in Fig. 1. Tubes shall be made of thoroughly annealed heat-resistant glass. Volumetric graduation tolerances,based on air-free water at 20C, are given in Table 1. Detailed requirements for centrifuge tubes appear in Test Methods D96 andD1796.7.2 Cooling Coil and Cooling Bath, a minimum length of6
23、mof5to7-mm outside diameter copper tubing wound to a diameterof 63.5 6 1.5-mm outside diameter, and assembled in a suitable cooling bath. (See Fig. 2 as an example.)7.2.1 Mechanical refrigeration is permitted provided that the coolant temperature is below 43C.43C. If dry ice is used, anon-glass dewa
24、r or vessel is recommended.7.3 Syringe, 2-mL graduated in 0.1 mL and equipped with a needle 200 6 5 mm long. The needle may be either a sharp needle(ordinary medical syringe needle) or a safe, non-sharp syringe needle to avoid a puncture hazard.Alternatively, an equivalent liquiddispensing device ca
25、pable of delivering 0.1-mL increments may be used, such as a 0.1-mL pipette.7.4 Temperature Measuring Device, that is intrinsically safe, with accuracy equal to or better than Specification E1 or IPAppendixA or IPTest Methods -AppendixA shall be used. Thermometers conforming to Specification E1 or I
26、PAppendixA havebeen found to be satisfactory.Low Range 38C to + 50C IP 1C/ASTM 5Cor IP 2C/ASTM 6CHigh Range 20C to + 50C ASTM 57CNOTE 1When a thermometer or a water bath, or both, are not available, for example when conducting a field test, a satisfactory alternative forscreening purposes is to warm
27、 the tip of the centrifuge tube with the hand.7.4.1 For routine testing, a general purpose thermometer with 0.5C subdivisions and a maximum scale error of 0.5C may beused.7.5 Absorbent Paper, white, 125-mm at least 100-mm diameter. Medium grade,grade or rapid filter paper has been found to besatisfa
28、ctory. In this test method, the paper will be referred to as “filter paper.”7.6 Solvent Wash Bottle, typically polyethylene.7.7 Water Bath, controlled at 38 6 2C.7.8 Copper Wire, 1.6 6 0.1-mm diameter, 300 6 10-mm long.,1to2-mm diameter, at least 10 mm longer than the centrifugetubes height.7.9 Clam
29、p, suitable for holding the centrifuge tube during weathering.8. Reagents and Materials8.1 SolventHPLC-grade pentane or cyclopentane. Another grade of solvent may be used provided that it meets therequirements of 10.2.8.1.1 Although pentane is the preferred solvent for use in this test method, cyclo
30、pentane may be substituted for pentanewhenever the ambient temperature or altitude is too high to enable the convenient handling of pentane.8.1.2 Storage of solvent in a polyethylene wash bottle for several days contaminates the solvent. Therefore, do not use anysolvent that has remained in a polyet
31、hylene wash bottle for more than one day.9. Hazards9.1 Note that there is a significant fire hazard from LPG vapors, and since the boiling point of LPG can be as low as 41C,D2158 112there is a risk of freezing “burns.” Take appropriate safety precautions to prevent ignition or fire, and wear suitabl
32、e protectiveequipment to protect against skin contact with liquid or vaporizing LPG.9.2 Operators should wear a grounded antistatic wrist strap. The use of an antistatic floor mat and grounding the sample cylinderare also advised.FIG. 1 Cone-Shaped Centrifuge Tube, 203 mmTABLE 1 Centrifuge Tube Grad
33、uation TolerancesRange, mLScale, Division,mLLimit of Error,mL0.0 to 0.1 0.05 0.020.1 to 0.3 0.05 0.030.3 to 0.5 0.05 0.050.5 to 1.0 0.1 0.051.0to3.0 0.1 0.13.0to5.0 0.5 0.25.0 to 25.0 1.0 0.525.0 to 100.0 1.0 1.0D2158 11310. Preparation of Apparatus10.1 Wash all glassware that is to be used in the t
34、est in the selected solvent.10.2 Verification of cleanliness of glassware and solvent.10.2.1 Add 10 mL of a new sample of solvent to the centrifuge tube.10.2.2 Mark the center of the filter paper with a pencil or other non-pentane-soluble writing tool.10.2.3 Fill the syringe or equivalent liquid dis
35、pensing device (see 7.3) with a portion of the solvent drawn from the centrifugetube and direct 0.1-mL portions of the solvent to the mark on the paper.10.2.3.1 The solvent is added in 0.1-mL increments to confine the solvent ring to a circle about 30 to 35 mm in diameter. Thefilter paper should be
36、held level during the solvent addition. One method is to place it on a 250-mL beaker.10.2.4 Allow the solvent to evaporate for 2 min, and note the persistence of an oil ring.10.2.4.1 The presence of an oil ring shall be observed by holding the dry filter paper between the eye and a bright incandesce
37、ntlight or strong daylight.10.2.4.2 If no oil ring appears after 1.5 mL of solvent has been added, the solvent and glassware are satisfactory.10.2.4.3 The appearance of an oil ring indicates either improperly cleaned glassware or contaminated solvent.11. Procedure11.1 Residue Measurement:11.1.1Attac
38、h the cooling coil to the LPG sample source, cool the coil to below the boiling point of the sample, and flush thecoil and sampling line.11.1.2Rinse and cool the centrifuge tube with the material to be sampled and then fill it to the 100-mLmark with a representativesample of LPG.11.1.3Immediately in
39、sert the copper wire through a clean, slotted cork or a clean, loose-fitting plug of cotton or cleansing tissuein the mouth of the centrifuge tube. The wire helps to prevent superheating and resulting bumping (erratic or excessive boiling),and the cork (or plug) will keep out air or moisture while t
40、he sample is weathering.11.1.4If more than 10 mL of the sample is lost because of bumping, obtain a new sample and repeat the test.11.1.5NOTECoils in the drawing are extended for clarity.FIG. 2 Precooling EquipmentD2158 11411.1.1 If the LPG sample is expected to be clean, with no residues or contami
41、nants that could result in an oil stain, the proceduremay be performed without a cooling coil. However, if a residue or oil stain is detected using this screening procedure (that is, aresidue is measured at greater than or equal to 0.05 mLin 11.1.7, or an oil stain is generated with 1.5 mLof test so
42、lution in 11.2.4),the test shall be repeated using a cooling coil.11.1.2 Attach the cooling coil to the LPG sample source, cool the coil to below the boiling point of the sample, and flush thecoil and sampling line.11.1.3 Rinse and cool the centrifuge tube with the material to be sampled and then fi
43、ll it to the 100-mL mark with arepresentative sample of LPG.11.1.4 Immediately insert the copper wire through a clean, slotted cork or a clean, loose-fitting plug of cotton or cleansing tissuein the mouth of the centrifuge tube. The wire helps to prevent superheating and resulting bumping (erratic o
44、r excessive boiling),and the cork (or plug) will keep out air or moisture while the sample is weathering.11.1.5 If more than 10 mL of the sample is lost because of bumping, obtain a new sample and repeat the test.11.1.6 Allow the sample to weather, using artificial heating if the ambient temperature
45、 or type of sample requires it. If, whenweathering has ceased and the tube has reached ambient temperature, a visible residue remains, place the tip of the tube in a waterbath at 38C for 5 min.11.1.67 Record the volume of any remaining residue to the nearest 0.05 mL, and the presence of extraneous m
46、atter, if observed.11.1.78 Perform the oil stain observation described in 11.2 even if there is no apparent or visible residue in the centrifuge tube.Experience has shown that there can be a thin film of oil on the inner surface of the centrifuge tube that is difficult to see and doesnot give a meas
47、urable volume, but can still give a ring or stain in the Oil Stain Observation procedure.11.2 Oil Stain Observation:11.2.1 Add sufficient solvent to the centrifuge tube containing the residue described in 11.1.5 11.1.6 to restore the volume to10 mL. Add the solvent from the wash bottle and carefully
48、 wash down the sides of the tube. Stir well so that any residue at thebottom of the tube is dissolved uniformly in the solvent. Stirring with the syringe needle (see 7.3) or pipette has been foundsatisfactory. This mixture will be referred to as the solvent-residue mixture.11.2.2 Mark the center of
49、a clean white filter paper.11.2.3 Fill the syringe or equivalent liquid dispensing device (see 7.3), and direct 1.5 mL of the solvent-residue mixture at thecenter of the paper at an appropriate rate such that the wetted circle is maintained at about 30 to 35 mm in diameter. If desired,steps 11.2.3 and 11.2.4 may be omitted, and the test continued according to 11.2.5.11.2.4 After directing the entire 1.5 mL of residue solution onto the filter paper and at the end of a 2-min waiting period, if nooil ring persists when holding the dry filter paper b
